# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Andy Hor'
_publ_contact_author_email       ANDYHOR@NUS.EDU.SG

_publ_section_title              
;
Ethylene Trimerisation with [NNN]
Heteroscorpionate Pyrazolyl Cr(III) Catalysts:
Effect of Ligand Structure on Activity and Selectivity
;
loop_
_publ_author_name
'Andy Hor.'
'Ai-Fang Li.'
'Jun Zhang.'

data_8395
_database_code_depnum_ccdc_archive 'CCDC 711871'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H28 Cl3 Cr N6'
_chemical_formula_weight         522.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.0925(16)
_cell_length_b                   14.7579(19)
_cell_length_c                   14.0641(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.897(4)
_cell_angle_gamma                90.00
_cell_volume                     2436.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1646
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      21.40

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1084
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8533
_exptl_absorpt_correction_T_max  0.9525
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14077
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4298
_reflns_number_gt                3085
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+0.0436P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4298
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.1507
_refine_ls_wR_factor_gt          0.1382
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.82850(5) 0.60729(4) 0.70591(5) 0.0380(2) Uani 1 1 d . . .
Cl1 Cl 0.86389(10) 0.50754(7) 0.59167(10) 0.0610(4) Uani 1 1 d . . .
Cl2 Cl 0.66241(9) 0.53720(7) 0.71940(9) 0.0519(3) Uani 1 1 d . . .
Cl3 Cl 0.93731(10) 0.52814(8) 0.83720(9) 0.0587(4) Uani 1 1 d . . .
N1 N 0.7368(3) 0.6930(2) 0.5977(2) 0.0392(8) Uani 1 1 d . . .
N2 N 0.7676(3) 0.7829(2) 0.6009(2) 0.0389(8) Uani 1 1 d . . .
N3 N 0.9713(3) 0.6870(2) 0.6973(2) 0.0412(8) Uani 1 1 d . . .
N4 N 0.9593(3) 0.7804(2) 0.6928(2) 0.0410(8) Uani 1 1 d . . .
N5 N 0.8209(3) 0.7074(2) 0.8137(3) 0.0424(9) Uani 1 1 d . . .
H5N H 0.890(4) 0.703(3) 0.840(4) 0.064(16) Uiso 1 1 d . . .
C1 C 0.6622(4) 0.6828(3) 0.5106(3) 0.0436(10) Uani 1 1 d . . .
C2 C 0.6469(4) 0.7652(3) 0.4603(3) 0.0509(12) Uani 1 1 d . . .
H2 H 0.5998 0.7754 0.3984 0.061 Uiso 1 1 calc R . .
C3 C 0.7138(4) 0.8280(3) 0.5187(3) 0.0460(11) Uani 1 1 d . . .
C4 C 0.6056(4) 0.5950(3) 0.4762(4) 0.0642(14) Uani 1 1 d . . .
H4A H 0.6579 0.5565 0.4535 0.096 Uiso 1 1 calc R . .
H4B H 0.5399 0.6060 0.4237 0.096 Uiso 1 1 calc R . .
H4C H 0.5825 0.5658 0.5294 0.096 Uiso 1 1 calc R . .
C5 C 0.7297(5) 0.9258(3) 0.5035(4) 0.0610(14) Uani 1 1 d . . .
H5A H 0.7098 0.9597 0.5553 0.092 Uiso 1 1 calc R . .
H5B H 0.6817 0.9441 0.4418 0.092 Uiso 1 1 calc R . .
H5C H 0.8079 0.9373 0.5036 0.092 Uiso 1 1 calc R . .
C6 C 0.8469(3) 0.8180(3) 0.6867(3) 0.0370(9) Uani 1 1 d . . .
H6 H 0.8520 0.8836 0.6781 0.044 Uiso 1 1 calc R . .
C7 C 1.0567(4) 0.8210(3) 0.6846(3) 0.0494(11) Uani 1 1 d . . .
C8 C 1.1330(4) 0.7536(3) 0.6858(3) 0.0548(12) Uani 1 1 d . . .
H8 H 1.2082 0.7608 0.6819 0.066 Uiso 1 1 calc R . .
C9 C 1.0792(4) 0.6719(3) 0.6937(3) 0.0470(11) Uani 1 1 d . . .
C10 C 1.0662(5) 0.9212(3) 0.6732(4) 0.0721(16) Uani 1 1 d . . .
H10A H 1.0283 0.9384 0.6076 0.108 Uiso 1 1 calc R . .
H10B H 1.1451 0.9380 0.6858 0.108 Uiso 1 1 calc R . .
H10C H 1.0313 0.9517 0.7188 0.108 Uiso 1 1 calc R . .
C11 C 1.1307(4) 0.5794(3) 0.6980(4) 0.0663(14) Uani 1 1 d . . .
H11A H 1.0956 0.5404 0.7369 0.099 Uiso 1 1 calc R . .
H11B H 1.2110 0.5832 0.7270 0.099 Uiso 1 1 calc R . .
H11C H 1.1186 0.5553 0.6329 0.099 Uiso 1 1 calc R . .
C12 C 0.8063(4) 0.8023(3) 0.7792(3) 0.0439(10) Uani 1 1 d . . .
H12A H 0.8483 0.8418 0.8304 0.053 Uiso 1 1 calc R . .
H12B H 0.7263 0.8184 0.7670 0.053 Uiso 1 1 calc R . .
C13 C 0.7565(4) 0.6894(3) 0.8912(3) 0.0461(11) Uani 1 1 d . . .
H13A H 0.6821 0.7178 0.8723 0.055 Uiso 1 1 calc R . .
H13B H 0.7452 0.6246 0.8961 0.055 Uiso 1 1 calc R . .
C14 C 0.8197(4) 0.7253(3) 0.9887(3) 0.0406(10) Uani 1 1 d . . .
C15 C 0.8106(4) 0.8149(3) 1.0166(3) 0.0516(12) Uani 1 1 d . . .
H15 H 0.7597 0.8537 0.9758 0.062 Uiso 1 1 calc R . .
C16 C 0.8763(5) 0.8467(3) 1.1038(4) 0.0616(14) Uani 1 1 d . . .
H16 H 0.8719 0.9073 1.1204 0.074 Uiso 1 1 calc R . .
C17 C 0.9484(5) 0.7892(4) 1.1666(4) 0.0639(14) Uani 1 1 d . . .
H17 H 0.9925 0.8109 1.2257 0.077 Uiso 1 1 calc R . .
C18 C 0.9553(4) 0.7005(3) 1.1420(4) 0.0591(13) Uani 1 1 d . . .
H18 H 1.0022 0.6611 1.1853 0.071 Uiso 1 1 calc R . .
C19 C 0.8930(4) 0.6692(3) 1.0533(3) 0.0506(12) Uani 1 1 d . . .
H19 H 0.9003 0.6089 1.0364 0.061 Uiso 1 1 calc R . .
N1S N 0.9635(7) 0.8444(6) 0.4294(5) 0.134(3) Uani 1 1 d . . .
C1S C 0.9490(7) 0.7689(6) 0.4246(5) 0.100(3) Uani 1 1 d . . .
C2S C 0.9250(7) 0.6738(5) 0.4124(6) 0.127(3) Uani 1 1 d . . .
H2S1 H 0.8572 0.6651 0.3613 0.190 Uiso 1 1 calc R . .
H2S2 H 0.9139 0.6491 0.4725 0.190 Uiso 1 1 calc R . .
H2S3 H 0.9878 0.6438 0.3950 0.190 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cr1 0.0385(4) 0.0278(3) 0.0474(4) 0.0003(3) 0.0097(3) 0.0001(3)
Cl1 0.0594(7) 0.0457(6) 0.0794(9) -0.0219(6) 0.0199(7) 0.0002(5)
Cl2 0.0470(6) 0.0383(6) 0.0707(8) 0.0039(5) 0.0147(6) -0.0076(5)
Cl3 0.0576(7) 0.0501(7) 0.0655(8) 0.0175(6) 0.0091(6) 0.0134(5)
N1 0.044(2) 0.0323(18) 0.041(2) -0.0004(15) 0.0099(17) -0.0007(15)
N2 0.049(2) 0.0341(18) 0.0325(19) 0.0003(14) 0.0071(16) 0.0025(15)
N3 0.040(2) 0.0311(18) 0.053(2) -0.0009(15) 0.0123(17) 0.0000(15)
N4 0.042(2) 0.0335(18) 0.049(2) -0.0016(15) 0.0141(17) -0.0015(15)
N5 0.046(2) 0.0367(19) 0.046(2) 0.0021(16) 0.0145(19) -0.0030(17)
C1 0.040(2) 0.049(2) 0.041(3) -0.006(2) 0.008(2) 0.004(2)
C2 0.046(3) 0.063(3) 0.039(3) 0.003(2) 0.002(2) 0.009(2)
C3 0.052(3) 0.040(2) 0.049(3) 0.004(2) 0.018(2) 0.012(2)
C4 0.065(3) 0.064(3) 0.057(3) -0.008(2) 0.001(3) -0.010(3)
C5 0.077(4) 0.047(3) 0.057(3) 0.015(2) 0.013(3) 0.011(2)
C6 0.046(3) 0.0268(19) 0.039(2) 0.0018(17) 0.0130(19) -0.0002(17)
C7 0.054(3) 0.049(3) 0.048(3) -0.008(2) 0.018(2) -0.012(2)
C8 0.037(2) 0.064(3) 0.066(3) -0.013(2) 0.018(2) -0.007(2)
C9 0.042(3) 0.048(3) 0.050(3) -0.001(2) 0.011(2) 0.000(2)
C10 0.072(4) 0.050(3) 0.104(4) 0.000(3) 0.040(3) -0.019(3)
C11 0.054(3) 0.055(3) 0.093(4) 0.005(3) 0.023(3) 0.010(2)
C12 0.060(3) 0.035(2) 0.038(2) -0.0019(18) 0.014(2) 0.004(2)
C13 0.048(3) 0.049(3) 0.044(3) 0.007(2) 0.017(2) -0.005(2)
C14 0.046(2) 0.039(2) 0.041(2) 0.0036(19) 0.021(2) -0.0006(19)
C15 0.068(3) 0.041(2) 0.052(3) 0.006(2) 0.026(2) 0.009(2)
C16 0.096(4) 0.036(2) 0.064(3) -0.009(2) 0.041(3) -0.010(3)
C17 0.071(3) 0.072(4) 0.050(3) -0.004(3) 0.016(3) -0.025(3)
C18 0.061(3) 0.058(3) 0.056(3) 0.012(2) 0.009(3) 0.003(2)
C19 0.063(3) 0.043(2) 0.047(3) 0.006(2) 0.015(2) 0.005(2)
N1S 0.165(7) 0.129(6) 0.133(6) -0.003(5) 0.082(5) 0.021(6)
C1S 0.120(6) 0.118(6) 0.082(5) 0.024(5) 0.062(4) 0.047(6)
C2S 0.134(7) 0.119(6) 0.149(7) 0.041(5) 0.077(6) 0.051(6)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 N1 2.082(3) . ?
Cr1 N3 2.117(3) . ?
Cr1 N5 2.134(4) . ?
Cr1 Cl1 2.2940(13) . ?
Cr1 Cl2 2.3072(13) . ?
Cr1 Cl3 2.3104(12) . ?
N1 C1 1.344(5) . ?
N1 N2 1.375(4) . ?
N2 C3 1.358(5) . ?
N2 C6 1.445(5) . ?
N3 C9 1.337(5) . ?
N3 N4 1.385(4) . ?
N4 C7 1.351(5) . ?
N4 C6 1.451(5) . ?
N5 C12 1.478(5) . ?
N5 C13 1.508(6) . ?
C1 C2 1.397(6) . ?
C1 C4 1.491(6) . ?
C2 C3 1.368(6) . ?
C3 C5 1.478(6) . ?
C6 C12 1.515(6) . ?
C7 C8 1.355(6) . ?
C7 C10 1.495(6) . ?
C8 C9 1.387(6) . ?
C9 C11 1.495(6) . ?
C13 C14 1.497(6) . ?
C14 C19 1.383(6) . ?
C14 C15 1.392(6) . ?
C15 C16 1.373(6) . ?
C16 C17 1.375(7) . ?
C17 C18 1.361(7) . ?
C18 C19 1.373(6) . ?
N1S C1S 1.127(10) . ?
C1S C2S 1.435(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cr1 N3 85.33(13) . . ?
N1 Cr1 N5 89.56(13) . . ?
N3 Cr1 N5 80.27(14) . . ?
N1 Cr1 Cl1 91.94(10) . . ?
N3 Cr1 Cl1 91.40(10) . . ?
N5 Cr1 Cl1 171.39(12) . . ?
N1 Cr1 Cl2 90.65(10) . . ?
N3 Cr1 Cl2 172.79(10) . . ?
N5 Cr1 Cl2 93.74(11) . . ?
Cl1 Cr1 Cl2 94.73(5) . . ?
N1 Cr1 Cl3 172.93(9) . . ?
N3 Cr1 Cl3 90.64(9) . . ?
N5 Cr1 Cl3 84.03(11) . . ?
Cl1 Cr1 Cl3 93.96(5) . . ?
Cl2 Cr1 Cl3 92.73(5) . . ?
C1 N1 N2 104.8(3) . . ?
C1 N1 Cr1 136.1(3) . . ?
N2 N1 Cr1 118.0(2) . . ?
C3 N2 N1 112.0(3) . . ?
C3 N2 C6 128.4(3) . . ?
N1 N2 C6 119.6(3) . . ?
C9 N3 N4 104.9(3) . . ?
C9 N3 Cr1 136.6(3) . . ?
N4 N3 Cr1 118.5(3) . . ?
C7 N4 N3 111.2(3) . . ?
C7 N4 C6 130.4(3) . . ?
N3 N4 C6 118.0(3) . . ?
C12 N5 C13 111.3(3) . . ?
C12 N5 Cr1 116.4(3) . . ?
C13 N5 Cr1 120.6(3) . . ?
N1 C1 C2 110.0(4) . . ?
N1 C1 C4 123.3(4) . . ?
C2 C1 C4 126.7(4) . . ?
C3 C2 C1 107.4(4) . . ?
N2 C3 C2 105.8(4) . . ?
N2 C3 C5 123.3(4) . . ?
C2 C3 C5 130.9(4) . . ?
N2 C6 N4 109.7(3) . . ?
N2 C6 C12 112.0(3) . . ?
N4 C6 C12 112.5(3) . . ?
N4 C7 C8 106.2(4) . . ?
N4 C7 C10 122.6(4) . . ?
C8 C7 C10 131.1(5) . . ?
C7 C8 C9 107.9(4) . . ?
N3 C9 C8 109.8(4) . . ?
N3 C9 C11 123.5(4) . . ?
C8 C9 C11 126.7(4) . . ?
N5 C12 C6 112.9(3) . . ?
C14 C13 N5 111.2(3) . . ?
C19 C14 C15 117.7(4) . . ?
C19 C14 C13 119.7(4) . . ?
C15 C14 C13 122.5(4) . . ?
C16 C15 C14 120.6(4) . . ?
C15 C16 C17 120.3(4) . . ?
C18 C17 C16 119.8(4) . . ?
C17 C18 C19 120.1(4) . . ?
C18 C19 C14 121.4(4) . . ?
N1S C1S C2S 176.1(10) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.078

# Attachment '8414.cif'

data_8414
_database_code_depnum_ccdc_archive 'CCDC 732288'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H35 Cl3 Cr Fe N7'
_chemical_formula_weight         671.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   11.0249(5)
_cell_length_b                   15.2942(6)
_cell_length_c                   18.2787(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3082.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    4106
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      22.39

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1388
_exptl_absorpt_coefficient_mu    1.113
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8248
_exptl_absorpt_correction_T_max  0.9362
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21834
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         27.50
_reflns_number_total             7065
_reflns_number_gt                5876
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.050(17)
_refine_ls_number_reflns         7065
_refine_ls_number_parameters     362
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.0882
_refine_ls_wR_factor_gt          0.0840
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.994
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.62624(5) 0.07569(3) 0.77282(3) 0.02562(12) Uani 1 1 d . . .
Fe1 Fe 0.67561(4) 0.32754(3) 1.04179(3) 0.02927(12) Uani 1 1 d . . .
Cl1 Cl 0.62572(9) -0.05342(5) 0.70692(5) 0.0362(2) Uani 1 1 d . . .
Cl2 Cl 0.50719(9) 0.01918(5) 0.86544(5) 0.0374(2) Uani 1 1 d . . .
Cl3 Cl 0.80331(9) 0.04174(5) 0.83440(5) 0.0399(2) Uani 1 1 d . . .
N1 N 0.4721(2) 0.12154(15) 0.71617(14) 0.0266(6) Uani 1 1 d . . .
N2 N 0.4767(2) 0.20309(16) 0.68479(14) 0.0277(6) Uani 1 1 d . . .
N3 N 0.7272(2) 0.14171(16) 0.69204(15) 0.0288(6) Uani 1 1 d . . .
N4 N 0.6875(3) 0.22301(15) 0.66979(14) 0.0278(6) Uani 1 1 d . . .
N5 N 0.6435(3) 0.19967(17) 0.82320(15) 0.0312(7) Uani 1 1 d . . .
H5N H 0.715(3) 0.211(2) 0.821(2) 0.027(10) Uiso 1 1 d . . .
C1 C 0.3660(3) 0.0881(2) 0.69353(18) 0.0318(7) Uani 1 1 d . . .
C2 C 0.3061(3) 0.1482(2) 0.6494(2) 0.0373(8) Uani 1 1 d . . .
H2 H 0.2298 0.1403 0.6274 0.045 Uiso 1 1 calc R . .
C3 C 0.3776(3) 0.2206(2) 0.64381(18) 0.0307(7) Uani 1 1 d . . .
C4 C 0.3204(4) 0.0002(2) 0.7157(2) 0.0416(9) Uani 1 1 d . . .
H4A H 0.3436 -0.0427 0.6792 0.062 Uiso 1 1 calc R . .
H4B H 0.2327 0.0018 0.7198 0.062 Uiso 1 1 calc R . .
H4C H 0.3552 -0.0158 0.7626 0.062 Uiso 1 1 calc R . .
C5 C 0.3594(4) 0.3050(2) 0.6049(2) 0.0409(9) Uani 1 1 d . . .
H5A H 0.3477 0.3514 0.6403 0.061 Uiso 1 1 calc R . .
H5B H 0.2885 0.3008 0.5736 0.061 Uiso 1 1 calc R . .
H5C H 0.4303 0.3177 0.5752 0.061 Uiso 1 1 calc R . .
C6 C 0.8283(3) 0.1268(2) 0.65303(19) 0.0357(8) Uani 1 1 d . . .
C7 C 0.8515(3) 0.1970(2) 0.6073(2) 0.0401(9) Uani 1 1 d . . .
H7 H 0.9169 0.2021 0.5745 0.048 Uiso 1 1 calc R . .
C8 C 0.7625(3) 0.2574(2) 0.61816(19) 0.0344(8) Uani 1 1 d . . .
C9 C 0.9027(4) 0.0463(2) 0.6607(2) 0.0518(11) Uani 1 1 d . . .
H9A H 0.9542 0.0513 0.7036 0.078 Uiso 1 1 calc R . .
H9B H 0.9527 0.0389 0.6175 0.078 Uiso 1 1 calc R . .
H9C H 0.8496 -0.0039 0.6661 0.078 Uiso 1 1 calc R . .
C10 C 0.7414(4) 0.3445(3) 0.5846(2) 0.0518(11) Uani 1 1 d . . .
H10A H 0.6644 0.3443 0.5589 0.078 Uiso 1 1 calc R . .
H10B H 0.8062 0.3575 0.5504 0.078 Uiso 1 1 calc R . .
H10C H 0.7397 0.3888 0.6227 0.078 Uiso 1 1 calc R . .
C11 C 0.5783(3) 0.25872(19) 0.70175(18) 0.0277(7) Uani 1 1 d . . .
H11 H 0.5632 0.3161 0.6784 0.033 Uiso 1 1 calc R . .
C12 C 0.5888(3) 0.27419(19) 0.78379(18) 0.0308(8) Uani 1 1 d . . .
H12A H 0.6383 0.3265 0.7923 0.037 Uiso 1 1 calc R . .
H12B H 0.5078 0.2854 0.8038 0.037 Uiso 1 1 calc R . .
C13 C 0.6233(4) 0.2076(2) 0.90420(18) 0.0361(8) Uani 1 1 d . . .
H13A H 0.5366 0.2007 0.9145 0.043 Uiso 1 1 calc R . .
H13B H 0.6666 0.1602 0.9291 0.043 Uiso 1 1 calc R . .
C14 C 0.6654(4) 0.2935(2) 0.93438(18) 0.0347(8) Uani 1 1 d . . .
C15 C 0.5931(4) 0.3683(2) 0.9483(2) 0.0490(11) Uani 1 1 d . . .
H15 H 0.5045 0.3731 0.9404 0.059 Uiso 1 1 calc R . .
C16 C 0.6696(6) 0.4348(3) 0.9766(2) 0.0628(14) Uani 1 1 d . . .
H16 H 0.6438 0.4942 0.9917 0.075 Uiso 1 1 calc R . .
C17 C 0.7876(6) 0.4018(3) 0.9798(2) 0.0680(16) Uani 1 1 d . . .
H17 H 0.8599 0.4338 0.9975 0.082 Uiso 1 1 calc R . .
C18 C 0.7858(4) 0.3153(3) 0.9545(2) 0.0502(10) Uani 1 1 d . . .
H18 H 0.8568 0.2760 0.9511 0.060 Uiso 1 1 calc R . .
C19 C 0.5485(4) 0.3066(3) 1.1206(2) 0.0495(10) Uani 1 1 d . . .
H19 H 0.4605 0.3184 1.1161 0.059 Uiso 1 1 calc R . .
C20 C 0.6071(4) 0.2282(2) 1.1026(2) 0.0436(9) Uani 1 1 d . . .
H20 H 0.5674 0.1749 1.0832 0.052 Uiso 1 1 calc R . .
C21 C 0.7309(4) 0.2379(3) 1.1165(2) 0.0492(10) Uani 1 1 d . . .
H21 H 0.7940 0.1928 1.1089 0.059 Uiso 1 1 calc R . .
C22 C 0.7506(4) 0.3241(3) 1.1433(2) 0.0505(10) Uani 1 1 d . . .
H22 H 0.8295 0.3496 1.1578 0.061 Uiso 1 1 calc R . .
C23 C 0.6371(4) 0.3662(3) 1.1456(2) 0.0486(10) Uani 1 1 d . . .
H23 H 0.6221 0.4270 1.1618 0.058 Uiso 1 1 calc R . .
N1S N -0.1282(4) 0.3276(3) 0.7707(2) 0.0688(11) Uani 1 1 d . . .
C1S C -0.0346(4) 0.3265(3) 0.7450(2) 0.0448(9) Uani 1 1 d . . .
C2S C 0.0859(4) 0.3217(3) 0.7119(2) 0.0539(11) Uani 1 1 d . . .
H2S1 H 0.1258 0.2683 0.7275 0.081 Uiso 1 1 calc R . .
H2S2 H 0.1336 0.3717 0.7273 0.081 Uiso 1 1 calc R . .
H2S3 H 0.0783 0.3219 0.6590 0.081 Uiso 1 1 calc R . .
N2S N 0.4452(4) 0.6737(4) 1.0037(3) 0.0825(14) Uani 1 1 d . . .
C3S C 0.3992(5) 0.6099(4) 0.9952(2) 0.0589(13) Uani 1 1 d . . .
C4S C 0.3379(6) 0.5251(3) 0.9854(3) 0.0773(16) Uani 1 1 d . . .
H4S1 H 0.3803 0.4806 1.0131 0.116 Uiso 1 1 calc R . .
H4S2 H 0.3381 0.5096 0.9340 0.116 Uiso 1 1 calc R . .
H4S3 H 0.2549 0.5295 1.0026 0.116 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cr1 0.0328(3) 0.0201(2) 0.0240(3) -0.0011(2) 0.0000(2) 0.0021(2)
Fe1 0.0311(3) 0.0314(2) 0.0254(2) -0.0046(2) -0.0022(2) 0.0003(2)
Cl1 0.0465(5) 0.0253(4) 0.0368(5) -0.0077(3) 0.0022(4) 0.0015(4)
Cl2 0.0499(5) 0.0285(4) 0.0338(4) 0.0039(4) 0.0103(4) 0.0009(4)
Cl3 0.0441(6) 0.0363(4) 0.0392(5) -0.0024(4) -0.0106(4) 0.0097(4)
N1 0.0324(15) 0.0201(12) 0.0272(14) -0.0016(11) 0.0003(12) 0.0020(11)
N2 0.0330(16) 0.0248(13) 0.0253(15) 0.0014(11) -0.0014(11) -0.0011(11)
N3 0.0316(16) 0.0276(14) 0.0274(15) -0.0013(12) -0.0004(12) 0.0001(11)
N4 0.0336(16) 0.0246(13) 0.0253(14) 0.0016(11) 0.0007(12) -0.0009(12)
N5 0.044(2) 0.0224(13) 0.0272(16) -0.0025(11) -0.0048(14) 0.0024(13)
C1 0.036(2) 0.0274(16) 0.0318(18) -0.0088(14) 0.0026(15) -0.0021(15)
C2 0.035(2) 0.0380(19) 0.039(2) -0.0058(16) -0.0071(17) -0.0004(15)
C3 0.0338(18) 0.0321(17) 0.0262(17) -0.0036(14) -0.0013(15) 0.0044(15)
C4 0.044(2) 0.0277(17) 0.053(2) -0.0036(17) 0.0021(19) -0.0081(15)
C5 0.043(2) 0.0389(19) 0.041(2) 0.0067(17) -0.0108(17) 0.0024(16)
C6 0.0360(19) 0.0381(18) 0.0329(19) -0.0050(16) 0.0027(16) -0.0022(15)
C7 0.039(2) 0.048(2) 0.034(2) -0.0032(17) 0.0107(16) -0.0049(16)
C8 0.040(2) 0.0374(18) 0.0256(18) -0.0005(15) 0.0001(15) -0.0107(16)
C9 0.044(3) 0.056(2) 0.055(3) -0.001(2) 0.0106(19) 0.0134(18)
C10 0.057(3) 0.050(2) 0.048(3) 0.016(2) 0.009(2) -0.004(2)
C11 0.0347(18) 0.0197(15) 0.0287(18) 0.0032(14) -0.0005(14) -0.0037(13)
C12 0.043(2) 0.0216(15) 0.0280(19) -0.0016(14) -0.0002(15) 0.0019(13)
C13 0.055(2) 0.0286(16) 0.0246(17) -0.0015(14) -0.0022(17) 0.0029(17)
C14 0.051(2) 0.0328(16) 0.0202(16) -0.0034(14) -0.0043(15) 0.0021(16)
C15 0.076(3) 0.0368(19) 0.035(2) -0.0095(17) -0.023(2) 0.0146(19)
C16 0.121(5) 0.028(2) 0.040(2) -0.0018(17) -0.018(3) -0.001(2)
C17 0.101(4) 0.068(3) 0.035(2) -0.010(2) 0.009(2) -0.049(3)
C18 0.047(2) 0.069(3) 0.035(2) -0.012(2) 0.0144(19) -0.010(2)
C19 0.034(2) 0.069(3) 0.045(2) -0.010(2) 0.0108(17) -0.0046(19)
C20 0.050(3) 0.045(2) 0.035(2) 0.0020(17) 0.0013(18) -0.0091(18)
C21 0.054(3) 0.053(2) 0.041(2) 0.013(2) -0.0106(19) 0.003(2)
C22 0.046(2) 0.073(3) 0.032(2) 0.002(2) -0.0083(17) -0.014(2)
C23 0.055(3) 0.059(2) 0.032(2) -0.0173(18) 0.0081(19) -0.013(2)
N1S 0.048(2) 0.100(3) 0.058(2) -0.014(2) -0.005(2) 0.014(2)
C1S 0.047(3) 0.047(2) 0.040(2) -0.0050(19) -0.0106(18) 0.0040(19)
C2S 0.054(3) 0.062(3) 0.045(2) 0.003(2) 0.0026(19) -0.010(2)
N2S 0.059(3) 0.119(4) 0.069(3) 0.007(3) -0.005(2) -0.016(3)
C3S 0.052(3) 0.094(4) 0.031(2) 0.006(3) 0.002(2) 0.016(3)
C4S 0.116(5) 0.072(3) 0.044(3) 0.000(2) -0.002(3) 0.026(3)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 N3 2.107(3) . ?
Cr1 N1 2.110(3) . ?
Cr1 N5 2.117(3) . ?
Cr1 Cl2 2.3100(10) . ?
Cr1 Cl3 2.3125(10) . ?
Cr1 Cl1 2.3130(9) . ?
Fe1 C18 2.014(4) . ?
Fe1 C17 2.024(4) . ?
Fe1 C16 2.029(4) . ?
Fe1 C20 2.029(4) . ?
Fe1 C21 2.030(4) . ?
Fe1 C22 2.032(4) . ?
Fe1 C23 2.033(4) . ?
Fe1 C15 2.033(4) . ?
Fe1 C14 2.034(3) . ?
Fe1 C19 2.035(4) . ?
N1 C1 1.341(4) . ?
N1 N2 1.374(3) . ?
N2 C3 1.352(4) . ?
N2 C11 1.440(4) . ?
N3 C6 1.343(4) . ?
N3 N4 1.379(3) . ?
N4 C8 1.360(4) . ?
N4 C11 1.446(4) . ?
N5 C12 1.477(4) . ?
N5 C13 1.502(4) . ?
C1 C2 1.389(5) . ?
C1 C4 1.493(4) . ?
C2 C3 1.363(5) . ?
C3 C5 1.488(4) . ?
C6 C7 1.384(5) . ?
C6 C9 1.487(5) . ?
C7 C8 1.362(5) . ?
C8 C10 1.486(5) . ?
C11 C12 1.523(5) . ?
C13 C14 1.498(5) . ?
C14 C18 1.417(5) . ?
C14 C15 1.417(5) . ?
C15 C16 1.419(6) . ?
C16 C17 1.396(7) . ?
C17 C18 1.402(6) . ?
C19 C20 1.402(5) . ?
C19 C23 1.411(5) . ?
C20 C21 1.397(5) . ?
C21 C22 1.423(6) . ?
C22 C23 1.408(6) . ?
N1S C1S 1.133(5) . ?
C1S C2S 1.462(6) . ?
N2S C3S 1.112(6) . ?
C3S C4S 1.472(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Cr1 N1 85.55(10) . . ?
N3 Cr1 N5 80.10(11) . . ?
N1 Cr1 N5 89.33(11) . . ?
N3 Cr1 Cl2 173.30(8) . . ?
N1 Cr1 Cl2 91.51(8) . . ?
N5 Cr1 Cl2 93.87(9) . . ?
N3 Cr1 Cl3 90.15(8) . . ?
N1 Cr1 Cl3 173.43(7) . . ?
N5 Cr1 Cl3 85.03(9) . . ?
Cl2 Cr1 Cl3 92.23(4) . . ?
N3 Cr1 Cl1 92.61(8) . . ?
N1 Cr1 Cl1 91.50(7) . . ?
N5 Cr1 Cl1 172.58(10) . . ?
Cl2 Cr1 Cl1 93.49(3) . . ?
Cl3 Cr1 Cl1 93.66(4) . . ?
C18 Fe1 C17 40.62(18) . . ?
C18 Fe1 C16 68.2(2) . . ?
C17 Fe1 C16 40.3(2) . . ?
C18 Fe1 C20 126.09(17) . . ?
C17 Fe1 C20 162.6(2) . . ?
C16 Fe1 C20 156.3(2) . . ?
C18 Fe1 C21 106.83(19) . . ?
C17 Fe1 C21 124.9(2) . . ?
C16 Fe1 C21 162.1(2) . . ?
C20 Fe1 C21 40.27(15) . . ?
C18 Fe1 C22 118.40(17) . . ?
C17 Fe1 C22 106.10(18) . . ?
C16 Fe1 C22 124.78(18) . . ?
C20 Fe1 C22 68.40(16) . . ?
C21 Fe1 C22 41.01(17) . . ?
C18 Fe1 C23 153.24(17) . . ?
C17 Fe1 C23 119.14(16) . . ?
C16 Fe1 C23 107.85(17) . . ?
C20 Fe1 C23 68.18(16) . . ?
C21 Fe1 C23 68.31(18) . . ?
C22 Fe1 C23 40.55(17) . . ?
C18 Fe1 C15 68.44(18) . . ?
C17 Fe1 C15 68.3(2) . . ?
C16 Fe1 C15 40.89(17) . . ?
C20 Fe1 C15 121.55(17) . . ?
C21 Fe1 C15 155.13(16) . . ?
C22 Fe1 C15 163.17(16) . . ?
C23 Fe1 C15 127.00(17) . . ?
C18 Fe1 C14 40.98(15) . . ?
C17 Fe1 C14 68.75(15) . . ?
C16 Fe1 C14 68.81(14) . . ?
C20 Fe1 C14 108.43(15) . . ?
C21 Fe1 C14 119.57(16) . . ?
C22 Fe1 C14 153.78(16) . . ?
C23 Fe1 C14 164.56(17) . . ?
C15 Fe1 C14 40.79(14) . . ?
C18 Fe1 C19 164.05(17) . . ?
C17 Fe1 C19 154.7(2) . . ?
C16 Fe1 C19 121.4(2) . . ?
C20 Fe1 C19 40.35(16) . . ?
C21 Fe1 C19 67.91(18) . . ?
C22 Fe1 C19 68.27(16) . . ?
C23 Fe1 C19 40.60(15) . . ?
C15 Fe1 C19 109.57(18) . . ?
C14 Fe1 C19 127.21(16) . . ?
C1 N1 N2 104.5(3) . . ?
C1 N1 Cr1 136.6(2) . . ?
N2 N1 Cr1 118.5(2) . . ?
C3 N2 N1 112.4(3) . . ?
C3 N2 C11 129.1(3) . . ?
N1 N2 C11 118.4(3) . . ?
C6 N3 N4 105.0(3) . . ?
C6 N3 Cr1 136.9(2) . . ?
N4 N3 Cr1 118.1(2) . . ?
C8 N4 N3 111.1(3) . . ?
C8 N4 C11 129.8(3) . . ?
N3 N4 C11 119.1(2) . . ?
C12 N5 C13 111.0(3) . . ?
C12 N5 Cr1 116.3(2) . . ?
C13 N5 Cr1 119.2(2) . . ?
N1 C1 C2 110.0(3) . . ?
N1 C1 C4 123.6(3) . . ?
C2 C1 C4 126.4(3) . . ?
C3 C2 C1 107.8(3) . . ?
N2 C3 C2 105.4(3) . . ?
N2 C3 C5 123.1(3) . . ?
C2 C3 C5 131.6(3) . . ?
N3 C6 C7 110.1(3) . . ?
N3 C6 C9 123.2(3) . . ?
C7 C6 C9 126.7(3) . . ?
C8 C7 C6 107.7(3) . . ?
N4 C8 C7 106.1(3) . . ?
N4 C8 C10 122.5(3) . . ?
C7 C8 C10 131.4(3) . . ?
N2 C11 N4 109.7(2) . . ?
N2 C11 C12 111.3(3) . . ?
N4 C11 C12 113.2(3) . . ?
N5 C12 C11 113.1(3) . . ?
C14 C13 N5 112.8(3) . . ?
C18 C14 C15 106.8(3) . . ?
C18 C14 C13 126.3(3) . . ?
C15 C14 C13 126.9(4) . . ?
C18 C14 Fe1 68.8(2) . . ?
C15 C14 Fe1 69.6(2) . . ?
C13 C14 Fe1 126.7(2) . . ?
C14 C15 C16 108.1(4) . . ?
C14 C15 Fe1 69.6(2) . . ?
C16 C15 Fe1 69.4(2) . . ?
C17 C16 C15 108.0(4) . . ?
C17 C16 Fe1 69.7(2) . . ?
C15 C16 Fe1 69.7(2) . . ?
C16 C17 C18 108.3(4) . . ?
C16 C17 Fe1 70.0(3) . . ?
C18 C17 Fe1 69.3(2) . . ?
C17 C18 C14 108.7(4) . . ?
C17 C18 Fe1 70.1(2) . . ?
C14 C18 Fe1 70.3(2) . . ?
C20 C19 C23 108.0(4) . . ?
C20 C19 Fe1 69.6(2) . . ?
C23 C19 Fe1 69.6(2) . . ?
C21 C20 C19 108.4(4) . . ?
C21 C20 Fe1 69.9(2) . . ?
C19 C20 Fe1 70.1(2) . . ?
C20 C21 C22 108.1(4) . . ?
C20 C21 Fe1 69.8(2) . . ?
C22 C21 Fe1 69.6(2) . . ?
C23 C22 C21 107.3(4) . . ?
C23 C22 Fe1 69.8(2) . . ?
C21 C22 Fe1 69.4(2) . . ?
C22 C23 C19 108.1(4) . . ?
C22 C23 Fe1 69.7(2) . . ?
C19 C23 Fe1 69.8(2) . . ?
N1S C1S C2S 178.0(5) . . ?
N2S C3S C4S 179.0(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.066